Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Diisopropylethylamine → HCID 86693784, 화합물
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Diisopropylethylamine | HCID 81531 | — |
| 반응물 | (1S,2R)-2-aminocyclohexan-1-ol hydrochloride | HCID 17039400 | — |
| 반응물 | 2-Chloro-4-fluoro-3-methylbenzonitrile | HCID 44550971 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | HCID 86693784 | HCID 86693784 | 29.6% |
반응 단계
A mixture of 2-chloro-4-fluoro-3-methyl-benzonitrile (500 mg, 2.95 mmol), diisopropylethylamine (1.29 mL, 7.37 mmol), and (1S,2R)-2-aminocyclohexanol hydrochloride (670 mg, 4.42 mmol, Acros®) is microwaved using a CEM® microwave at 190° C. for 2 h and 180° C. for 4 h. The mixture is diluted with dichloromethane and washed with 1 N HCl. The aqueous layer is extracted again with dichloromethane. The combined organic phases are dried over sodium sulfate, filtered, and concentrated in vacuo. The resulting residue is purified using radial chromatography, eluting with 2% methanol/dichloromethane. The isolated product is recrystallized with ether and hexane to yield the title compound as a white solid (231 mg, 29%). LC-ES/MS m/z 265.0 (M+1).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08658693B2 |
| 출처 데이터셋 | uspto-grants-2014_02 |
| ORD ID | ord-7392c902ed19404883235588542a6b88 |
| 출처 메모 | uspto-grants-2014_02 |